Detailed Information on Publication Record
2011
Silicophosphate Gels by Nonhydrolytic Condensation Reactions
STÝSKALÍK, Aleš, David ŠKODA, Zdeněk MORAVEC, Craig E. BARNES, Jiří PINKAS et. al.Basic information
Original name
Silicophosphate Gels by Nonhydrolytic Condensation Reactions
Authors
STÝSKALÍK, Aleš (203 Czech Republic, belonging to the institution), David ŠKODA (203 Czech Republic, belonging to the institution), Zdeněk MORAVEC (203 Czech Republic, belonging to the institution), Craig E. BARNES (840 United States of America) and Jiří PINKAS (203 Czech Republic, guarantor, belonging to the institution)
Edition
Hybrid Materials 2011 Conference, Strasbourg, France, 2011
Other information
Language
English
Type of outcome
Konferenční abstrakt
Field of Study
10402 Inorganic and nuclear chemistry
Country of publisher
France
Confidentiality degree
není předmětem státního či obchodního tajemství
RIV identification code
RIV/00216224:14740/11:00074155
Organization unit
Central European Institute of Technology
Keywords in English
Silicophosphate; Gels; Non-hydrolytic
Tags
Tags
International impact, Reviewed
Změněno: 1/12/2014 02:36, prof. RNDr. Jiří Pinkas, Ph.D.
Abstract
V originále
Phosphosilicate gel materials are usually synthesized from aqueous phosphoric acid and silicon alkoxides by hydrolysis. A high hydrolytic instability of the Si-O-P bonds leads to the products that are actually silicagels impregnated by aqueous H3PO4. Their calcination then provides crystalline silicophosphate phases. We prepared phosphosilicate gels by an elimination of acetic acid esters in heterocondensation reactions between Si(OC(O)CH3)4 and OP(OSiMe3)3 in nonaqueous organic solvents. 3 Si(OC(O)CH3)4 + 4 OP(OSiMe3)3 = 12 CH3C(O)OSiMe3 + Si3P4O16 While the ester elimination from metal alkoxides and silicon tetraacetate was reported previously, its application to phosphoric acid esters is new. The nonhydrolytic ester elimination provides clear amorphous phosphosilicate gels at room temperature with a high surface area up to 450 m2 g-1. Trimethylsilylester of acetic acid was identified by NMR and GC/MS as the elimination byproduct. 29Si CPMAS NMR evidenced the presence of octahedral SiO6 groups that must be connected to phosphorus atoms and thus attest to the presence of the Si-O-P bonds in the green gel. The condensation degree was 75-82% as established by gravimetric method. Infrared spectroscopy shows that the surface of the prepared gel is covered with residual acetate and trimethylsiloxy reactive groups. We can selectively replace acetates by the reaction with substituted phenols. That can be used for further modification of the surface properties. Crystallization of the gels upon calcination was studied by thermal analysis TG/DSC/FT-IR and powder XRD methods.
Links
| ED1.1.00/02.0068, research and development project |
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| GA203/08/1111, research and development project |
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| LH11028, research and development project |
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